Pure elemental powders of Al, Fe and Cr corresponding to the compositions of Al
90–xFe
xCr
10 (x= 10, 25, 50) were mechanically alloyed by high-energy ball mill using a ball-to-powder weight ratio of 250:10. The structural evolution in these alloys was investigated by X-ray diffraction and transmission electron microscopy. Additionally, thermal stability of the mechanically-alloyed powders was tested by DSG. Amorphous phase was partially formed in Al
65 Fe
25Cr
10 and Al
4OFe
50Cr
10 mechanically-alloyed powders at the early stage of milling. Al
5(Fe, Cr)
2 and Al(Fe, Cr) compounds were formed in the middle stage of milling. In the last milling stage, a mixture of amorphous and nanocrystal was obtained in Al
80Fe
10Cr
10 and Al
65Fe
25Cr
10 mechanically-alloyed powders. Only nanocrystal was observed in Al
40Fe
50Cr
10 mechanically-alloyed powder after long time milling. The crystallization temperature of these amorphous phases is about 150 K higher than that of the amorphous phase in Al–25 at%Fe binary system. It is proposed that the existence of Al–Cr atomic cluster in the amorphous matrix can improve the thermal stability of the amorphous matrix.
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